Process of producing fermentable sugars from cellulosic materials.



Gr.` H. TOMLINSON. PROCESS 0F PRODUGIVNG FBRMBNTABLE SUGARS FRM CELLULOSIC MATERIALS.

APPLIGATION FILED D'EG. 7, 191]... 1

Patented Ju1y`16,'1912.

IQ/M? (111,868, issued May 31, 1900, to Alexander products, whichnot only preventtheisolation,l of the'dextrose in a l.technically pure lquality, but also very considerably retard UniTED sTATEs PATENT oEE-icE.

"GEORGE TOMLINSON, CHICAGO, ILLINOIS, ASSlGNOR-TO STANDARD ALCOHOL C OMPANY,OF NEW YORK, N. A CORPORATION OE MAINE. i

PROCESS OFPRODUCING FERMENTABLE SUGARS FROM CEL-'LULOSIC MTERIALS.

Continuation of application Serial No.

l vspeizication of Letters Patent.

Patenti-ed July 1c, 1912.

- 1911.- `serial No. 664,373.

To all whom, it may concern Be it known `that I, GEORGE H. TOMLIN- soN,-a subject of the King of. Great Britain,

residing at' Chicago, in lthe county of Cook 5 and Stateof Illinoisgliave invented certain ',iieWgand 'useful Improvements in Processes ofroducing Ferinentable Sugars from Cel- -iuiosiMaterialsl 0f which-the allowing-is ofthe linvention being the provision of a '-'uctfrom which -the contained fermentablev pigocess whereby the Wood-Waste may be convvetted rapidly and veconomically into a prodsugars can be quickly andcompletel eX- tractedin the form of a solution,-whicli 'is not only s uiliciently. concentrated for ferwhich is practically freefrom substances eX'- mentation withoutfurther evaporation, but

".- erting a retarding or' preventive effect .upon

ffermentatiom or contains'the same only in such Aproportion-.asv notto interfere` mate rially Witlithe fermentation. y

It hasbeen. heretofore asserted ,that the use I .i U.of dilute acids .exerting a strongly hydrolyziiig effect upon cellulose or ligno-cellulose ivvas impracticable as ,a commercial methodv for the production of fermei'itable .sugars .'-from WoodfW-as'tgffor the reason that there Awere necessarily produced, in- 'conunction -f with the true fermentable-'sugars, products interfering With the normal fermentation of" 's'iich sugars.' For example, in German Patent v 4 "Classen, it is stated: If' the inversion of Wood fibers is carried on in the presence of 4dilute sulfuric acid, withor Without the applicatioiiofsteam pressure, there result byor render impossibleits ferment-ation.

I have discovered thatunder tproper conditions -itispiracticable to invert Wood-.waste V or 'other cellulosic materials by the action of dilute sulfuric or other 'strongly .hydrolyz- .ing iniiieralaid,as hydrochloric acid, while avoiding the formation .in practically. objec-v ltionablegquantitics of" the in]urious or fermentation-inhibiting -byfproducts above rel ferred to. The advantages 'of the invention may also beisecuredlyvithother hydrolyzirig agents or acids, as for example clilorin, sul= furous acid or the like.

In order to secure the above Vresults it 'is practically essential thatI the charge of Woody; Waste should be quickly and uniformly heated tothe temperature proper for thello of this reaction, or after it has proceeded to the 4desired stage, the converted charge should bej\ quickly 'cooled to o-rl below the boiling point, -under normal atmospheric pressure; ofthe Iresulting sugar solution. AIn order thatthis result may be practically :reaction by which the. fernientable vsugars are formed, and that after the completion and economically attained the following con-v l ditions should be fulfilled.

(l) The charge should be introduced and .maintained in such freely .permeable condition that it can be quickly and uniformly7 heated to the 'proper temperature by the direct introduction of steam into the body of the charge, such direct introduction of steam continuing, as and When required, until the fermentable sugars are formed. '(2) Such prolonged agitation, particularly in rotary digesters, as would give rise to any pronounced flouring or extreme com- I minution of the 'Wood must be avoided, such comminution leading to collateral reactions resulting in the formation of icy-products which interfere both with tlie extraction of the fermentable sugars and with their sub- The properly di; gested particles are relatively ,hard 'and sequent fermentation.

granular, and are in condition to forni a bed or mass which is freely permeable to water and 'which yieldsits sugars readily `undfrA the usual conditions of diffusion.I 1

' (3) The conditions as regar-ds concentration and quantity of acid, and time and tem` 'perature of heating must be properly controlled, but may be varied, with mutual corL relation, Within considerable limits. (4) The digester-walls should possess in additonto the necessary acid-.resisting cliar.- acter, a marked heat-insulating and heat-re;

taining function, tliisbeingessciitial to securing thebest resultsin. the process; forjit ispossible thereby to avoid such c'ondensan tion of-steam as would interfere with the free-permeability and absorptivel condition vo'f the mass, and yto `effect such rapid'lieating and conversion of the 'charge that even when largeweights are subjected to a slow tum;

successive' charges and the parts of each individual charge.

It isfpractically essential that the treatment be applied to large masses of niaterial, comprising usually a" ton or more of wood-waste orequivalent substance. Such large .masses veectively retain the heat., and

' thus suppleinent'tlie action of the' heat-retaining digester-lining, and render it possible to maintain throughout the complete operation the necessary permeability o'ffthe mass.

the interior of the mass to be heated. prefere ably'tvhile the latter is in a state of motion.

Relatively dry steam is preferred.

In 'conformity to the foregoing conditions -the method may-be carried into eectas, folloivs: The digester consists of a large vessel, having a capacity of a ton or moreof saw'- dust, mounted for rotatiomprovided With-a manhole adapted to be hermetically'closed' after vthe introduction of the charge, and provided also-With a suitable inlet forA the admission of steam to the linteriori ofl the charge, with a valved 'outlet of -suiiiciei-it capacitytopermit a rapid reduction of the internalpressure .at the close of the conver- .35 shimand lwith the usual'indicators of pressure and.- teniperature. The digester ispreferably spherical or splieioidal ii-n shape, an isprovided with an interior acidrelsisting lining which should be of` considerable thickness and of a heat-insulating charac-V ter.' A suitable lining' for the purpose may comprise 'acid-'resisting briclzv setin and backed by a suitable acid-resisting cement, which for use with sulfuric or vsulfurous acid may comprise wholly or iii-part a mi);- ture of litharge -and thickness of the heateinsulating lining shouldbe sufficient, under all the conditions. prevent' 4such condenof the operation, to sation of' steam. as'w'ould result in submerging vthe 'massg or-.any considerable proporf tion of it. vEiiposedinetallic linings are not. .adapted to the purpose of this invention by u ckle or4 separate Afrom suitable-type of,

`in mv acid or -a it maybe introduced steam into the interior gaseousghydrolyzing with the current of of' the mass to be converted but when a nonvolatile acid is used,

it is preferred to meisten thea-material tube/ glycerin. The total' bidh heat-conductivity 'and u copending ap T o .'f '8,443, filed March 10,. heipre'sent application'is a tinuation. In case a volatile: agent is used,

.moisture is charged into the rotary digester of large capacity,

metal, and is internally 'body for marin in. ne

fixed, axially disposed, ..perf0ra edpi extending through-thetrnniiionf2,.an

tity andconcentrationofacid, are-to acon- 'temperature of 212o F., or above. 'drolyzing agent is then introduced, either in the mov-ing mass, i'until.'

ture contentisfattainedf fTheidi'gester is roconverted with the-acid' solution', either fore or after the material has been cha f into the digester. In the latter event .die acid solution may be introduced as .'a -spr'aji or showerinto the vapor space ofthe 7;) gester after the charge has been heated 212G- Fahrenheit or jaboi'e by the direct ape plication of steam. Means for operating-'iii this manner are shown in the accompaying drawing njlierein the figure is avertical, longitudinal section. As therein illustrated," the digester comprises a spheroidal vessel 1 'mounted for' rotation 3. The shell Il is 'of lined. with acid-resisting'biick 5 vset in a suitable acid-resisting cement 6. A movement vof rotation upon trunnions `2,

may be imparted-to the digest'er a Worm The steam 'should be introduced into A gear 7. 8 represents the manhole forgthe introg5 duction of Wood-'wasmand he' .converted product, and for the vapors. Steam charge is introduced-iii o'iti' interi ingblank anges at the'point- S-lfl'fand 12; Steam and vapors may-be. blown o ff through the arched pipe "113, perforatedin thevlpor space of thedigester as indicated. at 14, and? communicating through. fthe trunnion 3 Withf the manifold 15. Tliehydrolyzing agent or vacid'solution is introducedinto' the digester l through the pipe 16` extending througli'- the 190 arched pipe 13, and'terminating'in aspray 11 nozzle 17', in positionto discharge the 'hydro-' lyzing agent upon the surface-of the mass to beconverted. y i Suitable operating conditions' are as follimited to the specic'details recited, inasmuchfas'the several factors of time and temperature .of thetreatment and the quansiderable degree and Within reasonable lim f vits mutually convertible: food-Waste' lconsisting largely vtaining approximately `'fifty' -of sawdust. and usually conper cent. 'o and heated therein by steam applied throughv 'the axially disposed perforatedpipa to a.

-The h vthe fori-n of vapor W'ith'the` current of steam, 120,v for preferably' n'tlie for f-'a 'shower 'or sprayof acid 'solution upon surface-.fof

Y l 'dfl'concent'rae vtotal moistated slowly. hr'oughout the entire operathe temperature is maintained, byfdirect inthe interior of `the 106i lows', .it being understood that 'the' invent-ion' -is not- La freelyv permeable condition'to the direct -action 'of steam 'under suitablev pressure, in

a; closed vesselhaving an acid-resisting,-

`hea;tinslatig and heat-retaining lining.

. n The process of "producing jferm'entable sugars lfrom woodfwasteor'other `cellulosic rewmrterials, which l'cv;onsis'ts in heating the -Ina'ss,; 'in-ifa freelyl ermeabl'ejstateand, in

presence ,of z rs'uitab e liy'wlrolyzingy agent, by` the direct actionv of steaml'favdmitted to the 0. I contining the Condition 'fiomyvodwaste'and other cellulosic Corrections-iu tained throughout eraticn '1n an unsaturated and process-jot; ing ermentablej' raw materials, which consists in lieting'the 'mass, in a freely permeable lstate, bythe 2O hydrolyzingf `a'gent,`a'11d Vcontinuing thegheatin'g byv the direct' action of steam until theA fermentl.able sugars are ormed,and so confining the direct 'action of steam,'tliereafter disseminatng through it a suitable heat tllat'the= masslis maintained through- -Qoutthe entire operation in' n unsaturated land]alosorlrtive'condition.

in presence of two witnesses.

Titnesses JOHN P.v VOIGHT, l VjnrAN 'WrLnrAMs fo. o.' BILLINGS,

`lIn testimony whereof I alix my signature GEORGE H. TOMLINsoN.

v N herey'eertied that in Letters Patent No. 1,632,48, -f jmnted JulyV 16, the ppl-ietion George HL Tomlinson, ,OflChicagoyIllinois, for an l'xnprcyernent in "I.Processes`.of Producing. FerlnentaJale Sugars-'.- from Cellulosic Mterials errors'appear the printed' specification requiring .correction es follows: i l 5-line 74 ,gfcr tlxelv/o'r accompayingfread accompanying; psigej, line 112, lie-Word 1"" dgest'erl strike cut the comme and insert the word-having,- andA v Letters-Betreut shouldfbe: read: with these correctionstherein thatv the seine rny'confornl' to thev recordof the cas-e in the Patent 'Ocel' i 'l "S-,igvnedancliseled thistlidaycf October, A.V D., 1912.l

I Acting Oommz'ssz'oner of .Patentg 

